Etching Technique Research Articles

Demonstration of MOCVD based in situ etching of β-Ga2O3 using TEGa

In this work, we demonstrate an in situ etch technique for β-Ga2O3 inside a metalorganic chemical vapor deposition (MOCVD) reactor using triethylgallium (TEGa) as the etching agent. At sufficiently high substrate temperatures (Tsub), TEGa is introduced into the MOCVD reactor which undergoes pyrolysis, resulting in the deposition of Ga on the β-Ga2O3 surface. These Ga adatoms react with Ga2O3 to form gallium suboxide (Ga2O), which desorbs from the β-Ga2O3 surface resulting in the etching of the epilayer. MOCVD chamber parameters such as TEGa molar flow rate, substrate temperature, and chamber pressure were shown to be key in controlling the etch rate and surface morphology. A wide range of etch rates from ∼0.3 to 8.5 μm/h is demonstrated by varying the etch parameters. In addition, smooth surface morphology on (010) and (001) β-Ga2O3 substrates is also demonstrated. This new etch technique could enable damage free fabrication of 3D structures like fins and trenches, which are key components in many β-Ga2O3 device structures.

Inorganic perovskite-based active multifunctional integrated photonic devices

The development of highly efficient active integrated photonic circuits is crucial for advancing information and computing science. Lead halide perovskite semiconductors, with their exceptional optoelectronic properties, offer a promising platform for such devices. In this study, active micro multifunctional photonic devices were fabricated on monocrystalline CsPbBr3 perovskite thin films using a top-down etching technique with focused ion beams. The etched microwire exhibited a high-quality micro laser that could serve as a light source for integrated devices, facilitating angle-dependent effective propagation between coupled perovskite-microwire waveguides. Employing this strategy, multiple perovskite-based active integrated photonic devices were realized for the first time. These devices included a micro beam splitter that coherently separated lasing signals, an X-coupler performing transfer matrix functions with two distinguishable light sources, and a Mach-Zehnder interferometer manipulating the splitting and coalescence of coherent light beams. These results provide a proof-of-concept for active integrated functionalized photonic devices based on perovskite semiconductors, representing a promising avenue for practical applications in integrated optical chips.

Cobalt etched graphite felt electrode for enhanced removal of organic pollutant in aqueous solution with a solid polymer electrolyte.

In this study, cobalt etched graphite felt electrodes were produced using a simple etching technique. It was used in combination with a solid polymer electrolyte (SPE) for the degradation of the target contaminant Orange II by Electro-Fenton (EF) technique in low conductivity water. In this method, 94% of Orange II in low conductivity water was removed in 90min. The characterization analysis substantiates the hypothesis that the electrodes produced exhibit a three-dimensional porous structure, augmented defect concentration, and enhanced electron transfer capability. In addition, the potential reaction mechanism was inferred from the radical quenching experiments, and hydroxyl radicals (·OH) were deemed the main reactive substances. The combination of cobalt etched graphite felt electrodes with SPE demonstrates remarkable efficacy in the treatment of organic wastewater characterized by low electrical conductivity.

A novel synthesis from instability difference between SiC 3-C and 6-H crystal to form nanoparticles stems by alkali solution and its degrading various environmental pollutants

In this paper, the nano silicon carbide with different sizes was prepared without hydrofluoric acid by using simple milling and related low temperature etching process in normal pressure. Also, it was the first time verified that 3-C dominated crystalline form of polycrystalline silicon carbide is etched, leaving the 6-H silicon carbide crystalline form by the Raman spectra and HAADF-STEM (high-angle-annular dark-field scanning transmission electron microscopy) imaging that. The application of the alkali etching technique could precise control the partial structural transformation of silicon carbide crystals to a certain extent, which further expands the traditional crystal structure transformation process. In addition, this paper demonstrates the silicon carbide composites in photocatalytic removal of various organic pollutants from aqueous solutions. In the photo degradation of MB (Methylene Blue), the removal rate of the modified silicon carbide shown ten times as much as the commercial silicon carbide. The 1-h degradation efficiency was significantly higher in the 50 μL H2O2 system (100.0%, 86.8% and 89.9% removal of MB, Rhodamine B, Methyl Orange and Tetracycline hydrochloride, respectively). Furthermore, the unit spin concentrations of vacancy defects, superoxide radicals and hydroxyl radicals were quantitatively analyzed. The vacancy defects of the etched material were 1000 times higher than before, and the modified silicon carbide had higher transmittance to infrared and visible light. It strongly absorbs ultraviolet light. Conversely, the research on micron-sized silicon carbide loaded with Ag and Pt atoms found that it had a nitrogen fixation effect during the warming up process, in a nitrogen atmosphere.

Comparative analysis of X‐band FSS fabricated by inkjet printing and conventional etching technique

AbstractAn investigation of a single‐layer band‐stop frequency selective surface (FSS) is designed and analyzed for X‐band application. The proposed FSS design primarily involves a cross‐shaped conductive patch with four square slots on each corner, and it is fabricated on the 3D‐printed polylactic acid (PLA) substrate. The design is resonating at 12 GHz with an insertion loss greater than 60 dB. The 10 dB bandwidth of the designed structure is 8.3% with respect to the resonant frequency. The results show that the design has polarization‐independent and angle‐insensitive transmission characteristics for incidence angles up to 60°. The simulation is carried out using CST Microwave Studio Suite, and the results are obtained. The physical mechanism of the designed structure is evaluated using the surface current distribution. The designed FSS is fabricated using two techniques, namely inkjet printing and conventional etching. Finally, the measurements of the fabricated structure are done using a vector network analyzer setup.

Novel high-voltage cathode for aqueous zinc ion batteries: Porous K0.5VOPO4·1.5H2O with reversible solid-solution intercalation and conversion storage mechanism

Cathode materials that possess high output voltage, as well as those that can be mass-produced using facile techniques, are crucial for the advancement of aqueous zinc-ion battery (ZIBs) applications. Herein, we present for the first time a new porous K0.5VOPO4·1.5H2O polyanionic cathode (P-KVP) with high output voltage (above 1.2 V) that can be manufactured at room temperature using straightforward coprecipitation and etching techniques. The P-KVP cathode experiences anisotropic crystal plane expansion via a sequential solid-solution intercalation and phase conversion pathway throughout the Zn2+ storage process, as confirmed by in-situ synchrotron X-ray diffraction and ex-situ X-ray photoelectron spectroscopy. Similar to other layered vanadium-based polyanionic materials, the P-KVP cathode experiences a progressive decline in voltage during the cycle, which is demonstrated to be caused by the irreversible conversion into amorphous VOx. By introducing a new electrolyte containing Zn(OTF)2 to a mixed triethyl phosphate and water solution, it is possible to impede this irreversible conversion and obtain a high output voltage and longer cycle life by forming a P-rich cathode electrolyte interface layer. As a proof-of-concept, the flexible fiber-shaped ZIBs based on modified electrolyte woven into a fabric watch band can power an electronic watch, highlighting the application potential of P-KVP cathode.

Sandwich-Type Self-Healing Sensor with Multilevel for Motion Detection.

Real-time detection of various parts of the human body is crucial in medical monitoring and human-machine technology. However, existing self-healing flexible sensing materials are limited in real-life applications due to the weak stability of conductive networks and difficulty in balancing stretchability and self-healing properties. Therefore, the development of wearable flexible sensors with high sensitivity and fast response with self-healing properties is of great interest. In this paper, a novel multilevel self-healing polydimethylsiloxane (PDMS) material is proposed for enhanced sensing capabilities. The PDMS was designed to have multiple bonding mechanisms including hydrogen bonding, coordination bonding, disulfide bonding, and local covalent bonding. To further enhance its sensing properties, modified carbon nanotubes (CNTs) were embedded within the PDMS matrix using a solvent etching technique. This created a sandwich-type sensing material with improved stability and sensitivity. This self-healing flexible sensing material (self-healing efficiency = 70.1% at 80 °C and 6 h) has good mechanical properties (stretchability ≈413%, tensile strength ≈0.69 MPa), thermal conductivity, and electrical conductivity. It has ultrahigh sensitivity, which makes it possible to be manufactured as a multifunctional flexible sensor.

Internal Adaptation of Composite Fillings Made Using Universal Adhesives-A Micro-Computed Tomography Analysis.

This study aimed to evaluate internal tooth-filling interfaces of composite fillings made using universal adhesives using micro-computed tomography (µCT). Sixty class V cavities were randomly assigned into six groups: Peak Universal etch and rinse (PER), Peak Universal self-etch (PSE), Adhese Universal etch and rinse (AER), and Adhese Universal self-etch (ASE). Two further adhesives considered gold standards were used as control groups: OptiBond FL (OER) for the etch and rinse technique and Clearfil SE for the self-etch technique (CSE). All teeth were subjected to thermomechanical loading and four-year water storage. Next, they were analyzed using µCT to investigate the internal tooth-filling interfaces. The proportions between the gap volume (GV) at the tooth-filling interface and the volume of applied composite filling (FV), between the gap and cavity volumes (CV), and between the gap volumes at the tooth-filling interface of the external (EGV) and internal (IGV) parts were calculated. Adhese Universal achieved the significantly lowest gap-to-filling- and gap-to-cavity-volume ratios for both types of etching techniques comparing to those of the Peak Universal and control groups. Significant differences between the gaps in external and internal parts of the tooth-filling interface were only noted in the control groups. Internal gap formation and development at the tooth-filling interface depend on the material as well as the type of its application.

Micron-scale FETs of fully epitaxial perovskite oxides using chemical etching

Advent of high mobility perovskite oxide semiconductor BaSnO3 (BSO) has enabled all-perovskite oxide heterostructures such as 2DEGs and FETs. To date all-perovskite oxide device demonstrations have been focused on finding and integrating the compatible perovskite dielectric oxides such as polar LaInO3 and LaScO3 and non-polar BaHfO3 and SrHfO3. For these demonstrations the length scale of BSO-based heterostructure devices has been about 100 µm, primarily due to the use of stencil masks for patterning. In order to further reduce the length scale, we employed a top-down approach using both photolithography and chemical etching techniques to pattern FETs made entirely of perovskite oxide materials: Ba0.997La0.003SnO3 channel layer, degenerately doped Ba0.96La0.04SnO3 contact layer, and SrHfO3 gate oxide layer. FETs of 3 µm channel length were fabricated using hydrofluoric acid and aqua regia as etchants. The FET exhibits a mobility of 38.8 cm²/Vs, an on/off ratio of 5.06 × 107, and a drain current density of 6.05 × 10−2 mA/μm, consistent with our expectation. These findings demonstrate the feasibility of patterning BSO through photolithography and chemical etching while maintaining the subsequent epitaxial growth, suggesting that BSO can be employed in a broader range of applications as well as for more precise studies of its intrinsic properties.

Praseodymium-Doped Ge20In5Sb10Se65 Films Based on Argon Plasma Cosputtering for Infrared-Luminescent Integrated Photonic Circuits.

In this paper, we report on the infrared luminescence of amorphous praseodymium-doped Ge20In5Sb10Se65 waveguides, which can be used as infrared sources in photonic integrated circuits on silicon substrates. Amorphous chalcogenide thin films were deposited by radiofrequency magnetron cosputtering using an argon plasma whose deposition parameters were optimized for chalcogenide materials. The micropatterning as ridge waveguides of the chalcogenide cosputtered films was performed using photolithography and plasma-coupled reactive ion etching techniques. The influence of the rare earth concentration within those thin films on their optical properties and rare earth spectroscopic properties was investigated. Using an excitation wavelength of 1.55 μm, the mid-infrared luminescence of Pr3+ ions from 2.5 to 5.5 μm was clearly demonstrated for studied chalcogenide materials. A wide range of waveguide widths and doping ratios were tested, assessing the ability of the cosputtering technique to preserve the luminescence properties of the rare earth ions initially observed in the bulk glass through the thin-film deposition and patterning process.

Dentin adhesion of bulk-fill composites and universal adhesives in class I-cavities with high C-factor

ObjectivesThe aim of this study was to compare the dentin adhesion of bulk-fill composites in high C-factor class I-cavities before and after thermocycling to a control group using incremental layering technique. MethodsA standardized class I-cavity was prepared into 195 human molars, then different universal adhesives were applied either in self-etch or etch & rinse mode, and the cavity was filled according to each materials application protocol. The material combinations used were a conventional layered composite as control, the respective bulk-fill product, two other bulk-fill composites made by different manufacturers, with one of them being tested using two different polymerization times. Furthermore, one thermoviscous bulk-fill composite and one self-adhesive restorative were examined of which the latter can only be applied in self-etch mode. In each group the dentin adhesion to the cavity bottom was measured using microtensile bond strength test initially (24 h water storage) and after thermocycling. All results were statistically analyzed using STATA 17.0. ResultsThe statistical analysis showed significant differences between the control and the experimental groups (p < 0.001). The highest mean bond strength before (14.8 ± 10.7 MPa) and after aging (14.2 ± 11.5 MPa) was measured for the etch & rinse-control group. Among the bulk-fill groups, the etch & rinse technique consistently showed higher bond strengths. Bond strength of groups with shortened polymerization did not exceed 2.1 MPa. The bond strength of the self-adhesive restoration material was low before and after thermocycling (2.7 MPa/ 0.0 MPa). Groups with low bond strength values showed a high number of pre-testing-failures. ConclusionsBulk-fill materials used in high C-factor class I-cavities showed lower bond strength during self-etch application. The same applies for a shortened polymerization regime, which cannot be recommended for high C-factor cavities. Clinical significanceToday, a large variety of materials and application techniques can be used when placing an adhesive restoration. Whether new instead of established procedures should be applied in high C-factor cavities has to be critically assessed, as they are a demanding scenario for adhesive restorations.

A Study on the Surface Quality and Damage Properties of Single-Crystal Silicon Using Different Post-Treatment Processes.

Detecting subsurface defects in optical components has always been challenging. This study utilizes laser scattering and photothermal weak absorption techniques to detect surface and subsurface nano-damage precursors of single-crystal silicon components. Based on laser scattering and photothermal weak absorption techniques, we successfully establish the relationship between damage precursors and laser damage resistance. The photothermal absorption level is used as an important parameter to measure the damage resistance threshold of optical elements. Single-crystal silicon elements are processed and post-processed optimally. This research employs dry etching and wet etching techniques to effectively eliminate damage precursors from optical components. Additionally, detection techniques are utilized to comprehensively characterize these components, resulting in the successful identification of optimal damage precursor removal methods for various polishing types of single-crystal silicon components. Consequently, this method efficiently enhances the damage thresholds of optical components.

Hydrogen and temperature measurement using a functionalized superstructure of Bragg gratings in a helical-core fiber

As decarbonization is urgent in global climate, hydrogen, of which the product is pure water after burning, becomes a potentially clean and sustainable energy source as a replacement for fossil fuels. However, the hydrogen storge is challenging due to the highly flammable and explosive properties, limiting its enormous applications in industries. Real-time and sensitive detection of hydrogen is thus imperative to avoid leakage accidents, while the sensors based on electric signals have the risk of spark or arc discharge which may induce explosion. Here, we propose and experimentally demonstrate an optical hydrogen sensor using a functionalized superstructure of Bragg gratings in a helical-core fiber with a thin palladium film. Due to the cross sensing of the two sets of gratings, simultaneous detection of hydrogen concentration and temperature can be realized. By modifying the device diameter using wet etching technique, the sensitivity of hydrogen concentration is enhanced by 2.7 times. The utilization of the superstructure of Bragg gratings sampled in the helical-core fiber provides a promising platform for reliable and safe sensing of hydrogen with the ability of simultaneous monitoring of temperature.

To evaluate the effect of different enamel conditioning procedures on the shear bond strength of new metal bracket on previously debonded tooth surface - An in-vitro study

To evaluate the efficacy of different enamel conditioning methods while bonding a new bracket on a previously de-bonded site, and assess the difference in shear bond strength and ARI score if any. 125 human-extracted premolars were selected. 250 premolar brackets were procured. 125 brackets were bonded on the buccal surface of the premolars using different enamel conditioning methods (bonding sequence 1) and was followed by debonding using the Instron Universal testing machine (Debonding procedure I).The remaining 125 brackets were bonded (Bonding sequence II) on the same teeth after the removal of residual adhesive. Bonding sequence II was followed by debonding (Debonding procedure II), shear bond strength calculation, and ARI score calculation. There was a significant difference in SBS between the 5 groups after initial debonding. SEP group (group 4) showed the highest SBS followed by acid etching groups (groups 3, 2, and 1). The sandblasting group (group 5) had the lowest shear bond strength value. After the second debonding, SBS was found to be highest in Group 3 {37% o-phosphoric acid (Bonding I) sandblasting (Bonding II)} followed by Group 4 {SEP (Bonding I and Bonding II)}, group 2 {acid etching (Bonding I) SEP (Bonding II)}, and group 1 (acid etching in both bonding sequences). Group 5 (sandblasting in both sequences) had the least SBS. Non-significant differences were found in ARI score of the five groups. Self-etching primer group had highest SBS and sandblasting group had least SBS after first debond. The SBS of new brackets after two debonding procedures significantly decreased but was still found to be above the required bond strength. SEP and sandblasting can be used as a substitute to acid etching technique in second time bonding of brackets as these groups had higher SBS after second debond.

One-step Cu-assisted chemical etching at room temperature of inverted pyramid array for high-performance crystalline silicon solar cells

Previous studies on the one-step Cu-assisted texturization of silicon wafers have predominantly focused on etching conditions at relatively high temperatures, which are unsuitable for the mass production of solar cells in industrial settings. In this study, we introduced the one-step Cu-assisted chemical etching (Cu-ACE) technique at room temperature to obtain large-area silicon inverted pyramid (IP) array structures. Based on this structure, diamond wire saw (DWS) mc-Si solar cells can achieve a balance between enhanced light trapping and lower carrier recombination by optimizing the concentration of the component Cu(NO3)2/HF/H2O2 in the etchant solution and the etching time during the Cu-ACE process. As a result, these solar cells deliver a power conversion efficiency (PCE) of 18.20 %, which is 1.99 % absolute higher than solar cells using traditional etching techniques. This work paves a new pathway toward the mass production of high-efficiency crystalline Si solar cells, offering a cost-effective and simple texturization approach.

Large area nanoscale patterning of functional materials using organosilicate ink based nanotransfer printing

This paper presents a versatile nanotransfer printing method for achieving large-area sub-micron patterns of functional materials. Organosilicate ink formulations combined with effective release layers have been shown to facilitate patterning of materials through the commonly used patterning approaches—lift off, physical etching and chemical etching. In this paper, we demonstrate that organosilicate ink formulations function as an effective resist owing to its superior physico-chemical stability whereas the release layers ensure clean removal of the resist post patterning. We successfully demonstrate patterning of sub-micron structures (800 nm feature sizes) of chromium metal through the lift off approach, silicon through reactive ion etching technique and silicon dioxide through wet chemical etching technique illustrating the versatility of the reported method. This patterning methodology represents a significant advancement in enabling nanostructure fabrication within resource-constrained laboratories. The approach requires nothing more than a master mold containing the desired structures, a spin coater, a low-temperature hotplate, and a desktop reactive ion etch tool.

Depth Analyses of Mg‐Acceptor and Si‐Donor Concentrations in GaN by Combining Stepwise Etching and Photoluminescence

The depth profiles of the Mg‐acceptor or Si‐donor concentration in GaN are visualized using stepwise etching and photoluminescence (PL) measurements. Low‐damage etching techniques are applied: multistep‐bias inductively coupled plasma reactive ion etching for p‐type GaN and electrochemical etching for n‐type GaN. To determine the concentration calibration curve, the PL intensity ratios of Mg‐neutral acceptor or Si‐neutral donor‐bound excitons to free excitons are plotted against Mg or Si atomic concentrations in etched GaN epitaxial layers having depth distributions of dopant concentrations, as estimated by secondary ion mass spectrometry. The quantitative accuracy of the calibration curve is ensured by the appropriate sample temperature and excitation density ranges for PL. The stepwise dry etching and the Mg acceptor quantification by PL using this calibration curve are applied to Mg‐ion‐implanted GaN after ultra‐high‐pressure annealing at 1300 °C for 1 min. The obtained depth profile of the Mg‐acceptor concentration is consistent with the Mg atomic concentration profile in the region deeper than the implantation peak, whereas the acceptor concentration in the shallow region is lower than the Mg atomic concentration. This analysis is useful for revealing the site substitution ratio of dopants in GaN materials partially involving inactive dopants.

Tunable Periodic Nanopillar Array for MAPbI3 Perovskite Photodetectors with Improved Light Absorption.

In the field of optoelectronic applications, the vigorous development of organic-inorganic hybrid perovskite materials, such as methylammonium lead triiodide (MAPbI3), has spurred continuous research on methods to enhance the photodetection performance. Periodic nanoarrays can effectively improve the light absorption of perovskite thin films. However, there are still challenges in fabricating tunable periodic patterned and large-area perovskite nanoarrays. In this study, we present a cost-effective and facile approach utilizing nanosphere lithography and dry etching techniques to create a large-area Si nanopillar array, which is employed for patterning MAPbI3 thin films. The scanning electron microscopy (SEM) and X-ray diffraction (XRD) results reveal that the introduction of nanopillar structures did not have a significant adverse effect on the crystallinity of the MAPbI3 thin film. Light absorption tests and optical simulations indicate that the nanopillar array enhances the light intensity within the perovskite films, leading to photodetectors with a responsivity of 11.2 A/W and a detectivity of 7.3 × 1010 Jones at 450 nm in wavelength. Compared with photodetectors without nanostructures, these photodetectors exhibit better visible light absorption. Finally, we demonstrate the application of these photodetector arrays in a prototype image sensor.

High-pressure plasma etching up to 9 atm toward uniform processing inside narrow grooves of high-precision X-ray crystal optics

We developed a new etching technique using plasma generated at high pressure up to 9 atm. Operating at 9-atm pressure with a 30-μm-diameter wire electrode, we demonstrated the generation of well-ordered plasma at a narrow gap of ∼10 μm between the electrode and workpiece, and realized a high spatial resolution of <40 μm during processing. This technique should allow for the processing of high-precision X-ray crystal optical devices with compact and complex structures, such as a micro channel-cut crystal monochromator with an extremely narrow (sub-100 μm width) groove for realization of Fourier-transform-limited X-ray lasers with high intensity.

Comparative in-vivo bond failure rate of orthodontic brackets when bracket base is treated with micro-abrasive blasting vs. acid etching: eighteen month randomized control trial and scanning electron microscope study.

The aim of this study was threefold. Firstly, it aimed to introduce and detail a novel method for chemically etching the bases of stainless-steel orthodontic brackets. Secondly, the study sought to investigate the structural alterations within the brackets' microstructure following chemical etching compared to those with sandblasted bases, using electron microscopy analysis. Lastly, the study aimed to evaluate and compare the long-term durability and survivability of orthodontic brackets with chemically etched bases versus those with sandblasted bases, both bonded using the conventional acid etch technique with Transbond XT adhesive, over an 18-month follow-up period. The study was a randomized clinical control trial with triple blinding and split-mouth study design and consisted of two groups. The brackets in the sandblasted group were prepared by sandblasting the intaglio surface of the base of the bracket with 50 µm SiO2 particles. Hydrofluoric acid was used to roughen the base in the acid-etched group. The bases of the brackets were viewed under an electron microscope to analyze the topographical changes. A total of 5,803 brackets (3,006 acid-etch, 2,797 sandblasted) in 310 patients were bonded, in a split-mouth design by the same operator. The patients were followed for 18 months. The failure rate of 2.59% and 2.7% was noted in an acid-etched and sandblasted group, respectively. There was a close approximation of curves in the Kaplan-Meier plot, and the survival distribution of the two groups in the log-rank (Mantel-Cox) test was insignificant; x2 = 0.062 (P value = 0.804). Acid etching if the bases of the brackets can be used as an alternative to sandblasting furthermore acid etching can be performed on the chair side.